CN102623687A - Preparation method for high-capacity molybdenum dioxide anode material and application of high-capacity molybdenum dioxide anode material - Google Patents
Preparation method for high-capacity molybdenum dioxide anode material and application of high-capacity molybdenum dioxide anode material Download PDFInfo
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- CN102623687A CN102623687A CN2012101004941A CN201210100494A CN102623687A CN 102623687 A CN102623687 A CN 102623687A CN 2012101004941 A CN2012101004941 A CN 2012101004941A CN 201210100494 A CN201210100494 A CN 201210100494A CN 102623687 A CN102623687 A CN 102623687A
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Abstract
The invention discloses a preparation method for a high-capacity molybdenum dioxide anode material. The method comprises the following steps of: 1) mixing de-ionized water, absolute ethanol and the solution of polyvinyl alcohol, and adding ammonium molybdate according to 0.02 to 0.04 grams per millimeter to obtain a precursor solution; 2) obtaining composite nano-fibers of the ammonium molybdate and polyvinyl alcohol by using the precursor solution under the action of 8KV static high voltage; 3) stabilizing the obtained nano-fibers in air; and 4) reducing and carbonizing the stabilized nano-fibers at high temperature in a reducing gas atmosphere to obtain a molybdenum dioxide nano-fiber composite material with a carbon coating. The invention also discloses an anode material prepared by the method, an electrode plate prepared from the anode material and a button cell comprising the electrode plate. A molybdenum dioxide nano-fiber prepared by the method has the diameter of about 120 nanometers and a length capable of reaching several microns, and the thickness of the carbon coating is about 3 nanometers; and when used as a lithium ion battery anode material, the molybdenum dioxide nano-fiber has high specific capacity, high rate capability and long cycle life.
Description
Technical field
The present invention relates to the lithium ion battery field, be specifically related to a kind of preparation method and application thereof of high power capacity negative material.
Background technology
Lithium ion battery is because of advantages such as energy density is high, average open-circuit voltage is high and have extended cycle life have been widely used in moving, portable electronics.Advantage is widely used in consumer electronics sector but flexible packing lithium ion battery is because of its size flexible design, security performance be good etc.But it is also increasingly high that miniaturization of electronic products, lightening development require the energy density of lithium ion battery, also increasingly high to the capacity requirement of lithium ion battery electrode material, especially negative active core-shell material.
At present, commercial lithium ion battery negative material adopts graphite material more, but its theoretical capacity 372mAh/g only, and the low (1.5～1.7g/cm of compacted density
3), big limitations the further lifting of lithium ion battery energy density.
Molybdenum dioxide has high power capacity (838mAh/g), high compacted density (6.5g/cm because of it
3) and by broad research.People such as the L.C.Yang of Fudan University adopt the molybdenum dioxide negative material of the method preparation of high temperature reduction molybdenum trioxide, and capacity is 318mAh/g (Journal of Power Sources, 179 (2008): 357-360), can not satisfy the application of suitability for industrialized production only.
Summary of the invention
The present invention is directed to the deficiency of prior art, a kind of preparation method of high power capacity molybdenum dioxide negative material is provided, solve present negative material finite capacity, can not adapt to the problem of suitability for industrialized production.
Be the realization above-mentioned purpose, the preparation method of a kind of high power capacity molybdenum dioxide negative material provided by the invention, its key step is following:
1) is that 1: 1: 10 deionized water, absolute ethyl alcohol and 10% poly-vinyl alcohol solution mix with volume ratio, adds ammonium molybdate, obtain precursor solution by 0.02～0.04 grams per milliliter.
2) precursor solution becomes the composite nano fiber of ammonium molybdate and polyvinyl alcohol under 8 kilovolts high pressure effect.
3) nanofiber that obtains is stable in the air, stabilization process is with the programming rate to 180 of 1 ℃ of per minute ℃, is incubated 30 minutes, and then is raised to 300 ℃ with identical programming rate, is incubated 30 minutes.
4) nanofiber that will stablize 500～800 ℃ of high temperature reductions 4～12 hours in the reducing gas atmosphere of hydrogen-argon-mixed body obtain the molybdenum dioxide nano-fiber composite material of carbon coating layer.
Through the composite nano fiber of electrostatic spinning of the present invention and the two step molybdenum dioxide that carbon coating layer is arranged that obtain of heat treating process, because the joint effect of the molybdenum dioxide of the coating of carbon and nanoscale, this material has good storage lithium performance.
The invention has the advantages that:
The first, the molybdenum dioxide active material specific capacity of preparing is high, good rate capability;
The second, the molybdenum dioxide active material good cycling stability of preparing, enclosed pasture efficient is high;
The 3rd, the molybdenum dioxide active material of preparing has coating layer, has improved the electrical conductivity performance and the ionic conduction performance of active material;
The 4th, the preparation method is simple, is fit to large-scale production.
Description of drawings
Among Fig. 1, (a), (b) be the different amplification FESEM figure of ammonium molybdate and polyvinyl alcohol composite nano fiber; (c) be the FESEM figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged; (d) be the XRD figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged.
Among Fig. 2, (a), (b) be the different amplification TEM figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged; (c) be the electron diffraction pattern figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged; (d) be the HRTEM figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged.
Fig. 3 is the cyclic voltammogram that the molybdenum dioxide nanofiber of carbon coating layer is arranged.
Fig. 4 is the charging and discharging curve (electric current is 50mA/g) that the molybdenum dioxide nanofiber of carbon coating layer is arranged.
Fig. 5 is high rate performance and the cycle performance figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged.
Fig. 6 be do not have have carbon coating layer the high rate performance and the cycle performance figure of molybdenum dioxide particle.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention is elaborated.
Embodiment one
At first, with 1 gram ammonium molybdate, 4 ml deionized water, the poly-vinyl alcohol solution of 4 milliliters of absolute alcohols and 40 milliliter 10% mixes the precursor solution that obtains.
Secondly, precursor solution under 8 kilovolts electrostatic high-pressure effect, is become the composite nano fiber of ammonium molybdate and polyvinyl alcohol.
Then, the nanofiber that obtains is earlier stable in the air, and stabilization process is with the programming rate to 180 of 1 ℃ of per minute ℃, is incubated 30 minutes, and then is raised to 300 ℃ with identical programming rate, is incubated 30 minutes.
Among Fig. 1 (a), (b) be the different amplification FESEM figure of ammonium molybdate and polyvinyl alcohol composite nano fiber.The composite nano fiber that can find out the molybdenum dioxide that carbon coating layer is arranged that obtains through reduction under stable in the air and the reducing atmosphere has well kept good fibre structure.
At last, the nanofiber that will stablize again 600 ℃ of reduction and carbonizations 5 hours in hydrogen-argon-mixed atmosphere have obtained having the molybdenum dioxide composite fibre of carbon coating layer.
The molybdenum dioxide nanofiber of the carbon coating layer through method for preparing is a kind of good negative material, has very high discharge capacity.(c) is the FESEM figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged among Fig. 1, can find out that the composite nano fiber of the molybdenum dioxide that carbon coating layer is arranged that obtains through carbonization under the inert atmosphere has well kept good fibre structure.(d) is the XRD figure that the molybdenum dioxide nanofiber of carbon coating layer is arranged among Fig. 1, confirms that this sample is the pure phase of molybdenum dioxide.Fig. 2 (a) (b) is the TEM figure of the composite nano fiber of molybdenum dioxide that carbon coating layer is arranged, can find out clearly that the carbon coating layer about nanofiber is by the molybdenum dioxide particle of the 20 nanometers size of inside and outside 3 nanometers is formed.Fig. 2 (c) is corresponding SEAD figure and high-resolution-ration transmission electric-lens figure (d), and its result can both be well corresponding with XRD result.
The above-mentioned molybdenum dioxide nanofiber that carbon coating layer is arranged that obtains and conductive black, PTFE binding agent are mixed by 75: 20: 5 weight ratio, and process is colded pressing, the die-cut electrode slice of processing.As to electrode, is electrolyte with 1mol/L LiPF6/ (EC:DMC) with metal lithium sheet, and the charging/discharging voltage scope is 3.0～0.01V.
Fig. 3 is the cyclic voltammogram that the molybdenum dioxide nanofiber of carbon coating layer is arranged.Peak than broad is arranged in the 0.64V position when discharging first, and it is caused for the irreversible reduction of electrolyte and SEI film form.After circulation in, the molybdenum dioxide redox couple of 1.23/1.49V and 1.50/1.75V is all obviously visible, and curves overlapped property is better, shows that this material cycle performance in charge and discharge process is better.Fig. 4 is the charging and discharging curve of composite nano fiber under the electric current of 50mA/g that the molybdenum dioxide of carbon coating layer is arranged; Can see that discharge capacity is up to 923mAh/g first; The capacity of the discharge 600mAh/g that still has an appointment for the second time; Shown good reversible capacity, after circulation 50 circles, capacity has reached 731mAh/g; When electric current is increased to 100mA/g and 200mA/g, 50 times its capacity of circulation back is respectively 582mAh/g, and 430mAh/g shows that the material of embodiment one preparation has excellent cycle performance.
Embodiment two
With 1 gram ammonium molybdate, 4 ml deionized water, the poly-vinyl alcohol solution of 4 milliliters of absolute alcohols and 40 milliliter 10% mixes the precursor solution that obtains.Precursor solution becomes the composite nano fiber of ammonium molybdate and polyvinyl alcohol under 8 kilovolts electrostatic high-pressure effect.The nanofiber that obtains is earlier stable in the air, and stabilization process is with the programming rate to 180 of 1 ℃ of per minute ℃, is incubated 30 minutes, and then is raised to 300 ℃ with identical programming rate, is incubated 30 minutes.The 500 ℃ of carbonizations 12 hours in nitrogen atmosphere of the nanofiber that will stablize have again obtained having the molybdenum dioxide composite fibre of carbon coating layer.
With the above-mentioned molybdenum dioxide nanofiber that carbon coating layer is arranged that obtains by being assembled into button cell, the test point performance with embodiment one identical mode.
Embodiment three
With 2 gram ammonium molybdates, 8 ml deionized water, the poly-vinyl alcohol solution of 8 milliliters of absolute alcohols and 80 milliliter 10% mixes the precursor solution that obtains.Precursor solution becomes the composite nano fiber of ammonium molybdate and polyvinyl alcohol under 8 kilovolts electrostatic high-pressure effect.The nanofiber that obtains is earlier stable in the air, and stabilization process is with the programming rate to 180 of 1 ℃ of per minute ℃, is incubated 30 minutes, and then is raised to 300 ℃ with identical programming rate, is incubated 30 minutes.The 700 ℃ of carbonizations 4 hours in nitrogen atmosphere of the nanofiber that will stablize have again obtained having the molybdenum dioxide composite fibre of carbon coating layer.
With the above-mentioned molybdenum dioxide nanofiber that carbon coating layer is arranged that obtains by being assembled into button cell, the test point performance with embodiment one identical mode.
Embodiment four
With 2 gram ammonium molybdates, 8 ml deionized water, the poly-vinyl alcohol solution of 8 milliliters of absolute alcohols and 80 milliliter 10% mixes the precursor solution that obtains.Precursor solution becomes the composite nano fiber of ammonium molybdate and polyvinyl alcohol under 8 kilovolts electrostatic high-pressure effect.The nanofiber that obtains is earlier stable in the air, and stabilization process is with the programming rate to 180 of 1 ℃ of per minute ℃, is incubated 30 minutes, and then is raised to 300 ℃ with identical programming rate, is incubated 30 minutes.The 800 ℃ of carbonizations 4 hours in the nitrogen mixture atmosphere of the nanofiber that will stablize have again obtained having the molybdenum dioxide composite fibre of carbon coating layer.
With the above-mentioned molybdenum dioxide nanofiber that carbon coating layer is arranged that obtains by being assembled into button cell, the test point performance with embodiment one identical mode.
Among above-mentioned each embodiment, deionized water, absolute alcohol and poly-vinyl alcohol solution only be exemplary with magnitude relation, be not confined on the above-mentioned consumption.In general, satisfy 1: 1: 10 volume ratio as long as satisfy the consumption of deionized water, absolute alcohol and poly-vinyl alcohol solution, the addition of ammonium molybdate is not limited in the content of the foregoing description yet, is preferably 0.02～0.04 grams per milliliter.Simultaneously, the concentration of poly-vinyl alcohol solution is generally 8%-10%, and electrostatic high-pressure is generally 8-12kV; In addition, in the aerial stabilization process, also be not limited to temperature and mode in the foregoing description; As long as can keep the one dimension fibre structure, certain content of organics gets final product.And in the step of carrying out carbonization, carburizing temperature can be selected according to actual needs, and in 500-800 ℃ of scope, carbonization time (like carburizing temperature etc.) according to actual needs can specifically be selected, as 4-12 hour.
Below in conjunction with a Comparative Examples, the effect with molybdenum dioxide negative material that carbon coats of the method preparation that utilizes various embodiments of the present invention is specifically described.
Comparative Examples:
The ammonium molybdate particle is handled through the heat treatment mode identical with embodiment one, and earlier stable in the air, stabilization process is with the programming rate to 180 of 1 ℃ of per minute ℃, is incubated 30 minutes, and then is raised to 300 ℃ with identical programming rate, is incubated 30 minutes.The 600 ℃ of carbonizations 5 hours in hydrogen-argon-mixed atmosphere of the particle that will stablize again obtain the molybdenum dioxide particle that does not have carbon to coat.The gained material by being assembled into button cell with embodiment one identical mode, is tested electrical property.
The electrical property contrast of table 1 embodiment and Comparative Examples battery
In sum, the composite nano fiber of the molybdenum dioxide that the preparation method of the molybdenum dioxide negative material that proposes according to the present invention prepares has good capacity and cycle performance, and the preparation method is simple, is fit to large-scale production.
Need to prove that according to the announcement and the elaboration of above-mentioned specification, those skilled in the art in the invention can also change and revise above-mentioned execution mode.Therefore, the embodiment that discloses and describe above the present invention is not limited to also should be in the protection range of claim of the present invention to equivalent modifications more of the present invention and change.In addition, although used some specific terms in this specification, these terms are explanation for ease just, the present invention is not constituted any restriction.
Claims (10)
1. the preparation method of a molybdenum dioxide negative material, key step is following:
1) configuration precursor solution
A certain proportion of deionized water, absolute ethyl alcohol and poly-vinyl alcohol solution are mixed, add ammonium molybdate again, obtain precursor solution;
2) said precursor solution is placed under the electrostatic high-pressure effect, make it become the composite nano fiber of ammonium molybdate and polyvinyl alcohol;
3) said composite nano fiber is carried out stabilized treatment;
4) the composite nano fiber high temperature reduction in reducing gas atmosphere after will stablizing promptly obtains the molybdenum dioxide nano-fiber composite material of carbon coating layer.
2. the preparation method of a kind of molybdenum dioxide negative material according to claim 1 is characterized in that, the deionized water in the said precursor solution, absolute ethyl alcohol and poly-vinyl alcohol solution volume ratio are 1: 1: 10.
3. according to the preparation method of a kind of molybdenum dioxide negative material described in claim 1 or 2, wherein, the amount of ammonium molybdate adds in the mixed solution by 0.02～0.04 grams per milliliter.
4. according to the preparation method of a kind of molybdenum dioxide negative material described in one of claim 1-3, wherein, said poly-vinyl alcohol solution concentration is 8%-10%.
5. according to the preparation method of a kind of molybdenum dioxide negative material described in one of claim 1-4, wherein, in the said high temperature reduction, reducing gas is hydrogen-argon-mixed body, and the high temperature reduction temperature is 500～800 ℃, and the time of high temperature reduction is 4～12 hours.
6. according to the preparation method of a kind of molybdenum dioxide negative material described in one of claim 1-5, wherein, said electrostatic high-pressure is preferably 8-12kV.
7. according to the preparation method of the described a kind of molybdenum dioxide negative material of one of claim 1-6; Wherein, described stabilized treatment is specially: with the programming rate to 180 of 1 ℃ of per minute ℃, be incubated 30 minutes; And then be raised to 300 ℃ with identical programming rate, be incubated 30 minutes.
8. the prepared molybdenum dioxide negative material of the described preparation method of one of claim 1-7.
9. electrode slice, it is mixed by 75: 20: 5 weight ratio by the described molybdenum dioxide negative material of claim 8 and conductive black, PTFE binding agent, through colding pressing, die-cut processing.
10. button cell, it comprises the described electrode slice of claim 9.
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Cited By (8)
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| CN102815749A (en) * | 2012-08-08 | 2012-12-12 | 西安工程大学 | Preparation method of molybdenum dioxide nanorod |
| CN105175965A (en) * | 2015-09-06 | 2015-12-23 | 安徽工业大学 | Lithium molybdate nano-rod electronic packaging material |
| CN106115785A (en) * | 2016-06-24 | 2016-11-16 | 陕西科技大学 | A kind of pure phase MoO2anode material of lithium-ion battery and preparation method thereof |
| WO2018108011A1 (en) * | 2016-12-15 | 2018-06-21 | 清华大学 | Method of manufacturing flexible transparent electrically conductive thin film, and product thereof |
| CN109081347A (en) * | 2018-07-16 | 2018-12-25 | 湖南大学 | A method of based on mutually separation synthesis porous carbon microsphere |
| CN109399722A (en) * | 2018-12-27 | 2019-03-01 | 陕西科技大学 | A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite |
| CN110042503A (en) * | 2019-05-08 | 2019-07-23 | 陕西科技大学 | A kind of MoSe2@C electrospinning hollow Nano fiber in use and its preparation method and application |
| CN111036095A (en) * | 2019-12-31 | 2020-04-21 | 济南大学 | Flexible self-supporting MoO2@ C nanofiber film material and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815749A (en) * | 2012-08-08 | 2012-12-12 | 西安工程大学 | Preparation method of molybdenum dioxide nanorod |
| CN105175965A (en) * | 2015-09-06 | 2015-12-23 | 安徽工业大学 | Lithium molybdate nano-rod electronic packaging material |
| CN106115785A (en) * | 2016-06-24 | 2016-11-16 | 陕西科技大学 | A kind of pure phase MoO2anode material of lithium-ion battery and preparation method thereof |
| WO2018108011A1 (en) * | 2016-12-15 | 2018-06-21 | 清华大学 | Method of manufacturing flexible transparent electrically conductive thin film, and product thereof |
| CN109081347A (en) * | 2018-07-16 | 2018-12-25 | 湖南大学 | A method of based on mutually separation synthesis porous carbon microsphere |
| CN109399722A (en) * | 2018-12-27 | 2019-03-01 | 陕西科技大学 | A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite |
| CN109399722B (en) * | 2018-12-27 | 2020-10-30 | 陕西科技大学 | Preparation method of porous rod-like molybdenum dioxide/carbon composite material |
| CN110042503A (en) * | 2019-05-08 | 2019-07-23 | 陕西科技大学 | A kind of MoSe2@C electrospinning hollow Nano fiber in use and its preparation method and application |
| CN110042503B (en) * | 2019-05-08 | 2021-06-22 | 陕西科技大学 | MoSe2@ C electrospun hollow nanofiber and preparation method and application thereof |
| CN111036095A (en) * | 2019-12-31 | 2020-04-21 | 济南大学 | Flexible self-supporting MoO2@ C nanofiber film material and preparation method and application thereof |
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Application publication date: 20120801 |